CN103043664B - Method and device for directionally solidifying and purifying polysilicon by vacuum extraction of tailing - Google Patents
Method and device for directionally solidifying and purifying polysilicon by vacuum extraction of tailing Download PDFInfo
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- CN103043664B CN103043664B CN201210537365.9A CN201210537365A CN103043664B CN 103043664 B CN103043664 B CN 103043664B CN 201210537365 A CN201210537365 A CN 201210537365A CN 103043664 B CN103043664 B CN 103043664B
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Abstract
The method comprises: in an inert gas, melting the silicon material to form silicon melt and insulating; directionally solidifying; stopping ingot pulling when 85-90% of melt is solidified, then diving a quartz tube into the residual silicon melt, vacuum-pumping the other end of the quartz tube by a vacuum-pumping device, pushing the residual silicon melt into the quartz tube under the action of pressure difference, continuously and downwards pulling the ingot, and diving a tailing collecting box below the quartz tube when a crucible departs from a heating zone; cutting off power supply, and stopping heating. After spalling, the quartz tube following the tailing falls down to the collecting box, and the ingot casting obtained in the crucible is high purity silicon ingot casting. The method and the device prevent the diffusion of impurity, reduce technology, and raise yield of the ingot casting. Direct separation of impurity enrichment region is implemented in an end stage of solidification. The device has advantages of convenient reconstruction and installation, and simple operation, can effectively removes the impurity enriched in the tail part of the ingot casting, and saves a production period and cost.
Description
Technical field
The invention belongs to metallurgy purification technical field, particularly a kind ofly extract the method and apparatus that tailing carries out directional solidification purified polysilicon.
Background technology
The development of photovoltaic industry depends on the purification to silicon raw material, in the process that silicon raw material is purified, directional solidification process is most important to removing the metallic impurity that in silicon raw material, segregation coefficient is very little, it is one of current solar-grade polysilicon effective means of purifying, in addition, directional solidification technique is widely used in metallurgy purification.Directional freeze is to adopt compulsory means in melt, to form the thermograde of specific direction, make the melt crystallization nucleation at the position that temperature is low, first the starting point that becomes melt solidifying solidifies, existence due to thermograde, melt solidifies along the contrary direction of hot-fluid, obtains the column crystal with specific orientation.It is to utilize the different solubility of impurity element in melt and solid that directional freeze is purified, the impurity element that segregation coefficient is less in process of setting is pushed to solid-liquid interface forward position, constantly enrichment in melt, and finally the afterbody at ingot casting solidifies, by the excision of ingot casting afterbody, can reach the object of purification.
Yet, ingot casting is solidifying coda, impurity enriched is in the melt at crucible top, in the end in slow solidification process, the impurity that content is high can be to the low position diffusion of foreign matter content, make silicon purity along with the prolongation of soaking time reduces on the contrary gradually, this has affected refining effect, and in this case, the afterbody tailing of excision is up to 25% ~ 35%, be that yield rate is only 65-75%, and the hardness ratio of silicon ingot is larger, need high-power cutting facility the silicon ingot of purification and the high ingot casting tailing of afterbody foreign matter content could be separated, the general method of line cutting and the cutting of diamond saw band of using is cut at present, but cutting facility cost is high, saw band consumption is large, be unfavorable for the reduction of industrial production cost, and domestic rarely seen fruitful method facilitates the removal of tailing.
Summary of the invention
The present invention seeks to as overcoming above deficiency, a kind of method that vacuum drawn tailing carries out directional solidification purified polysilicon has been proposed, solidifying coda, silica tube is stretched in the not solidified excess silicon melt in upper strata, utilize vacuum unit to vacuumize at the silica tube the other end, make between vacuum chamber and silica tube mineralization pressure poor, under the effect of pressure difference, upper strata melt is clamp-oned in silica tube, carry out aftertreatment and remove impurity tailing, realize the direct separation in impurity enriched district solidifying ending phase, effectively contained the back diffusion of impurity, reduced purifying technique, improved the yield of ingot casting, the equipment that utilizes the method to adopt has also been proposed in addition, this equipment is simple, easy and simple to handle, cost is lower, and being beneficial to the tailing that foreign matter content is high is removed quickly and easily.
The technical scheme that adopted is for achieving the above object: a kind of vacuum drawn tailing carries out the method for directional solidification purified polysilicon, it is characterized in that: in protection of inert gas environment, clean silicon material is heated to melt completely after forming silicon melt is incubated; Lower the temperature afterwards, draw ingot vertically downward, carry out directional freeze; When having solidified 85 ~ 90%, stop drawing ingot, silica tube is stretched in the not solidified excess silicon melt in upper strata, with vacuum unit, the silica tube the other end is vacuumized afterwards, the not solidified excess silicon melt in upper strata enters among silica tube under pressure difference effect, and until upper strata, not solidified excess silicon melt is all pressed into after silica tube, continues to pull down ingot, until crucible upper end, leave behind heating zone, tailing collection box is extended under silica tube; Cut off the electricity supply, stop heating, in silica tube, melt solidifying expands, and after silica tube spalling, with tailing, falls in tailing collection box, solidifies the ingot casting obtaining and be HIGH-PURITY SILICON ingot casting in crucible.
The concrete steps of the method that adopts are as follows:
The first step pre-treatment: add the clean silicon material of crucible volume 90 ~ 95% in crucible, close vent line, open vacuum pump group, first the vacuum tightness in vacuum chamber is extracted into 0.01-10Pa, close afterwards vacuum pump group, open vent line, in vacuum chamber, be filled with rare gas element, reach 100 ~ 4000Pa to pressure, close vent line;
Second step melting, solidify: power-on, utilize ruhmkorff coil and graphite heater that the silicon material in crucible is heated to 1450 ~ 1650 ℃ to being fused into silicon melt completely, and be incubated 30 ~ 60min at this temperature, pull vertically downward aqueous cold plate, make silicon melt in crucible with the speed of 0.1-2mm/min uniform motion vertically downward, draw ingot, silicon melt is carried out directional freeze to top by crucible bottom, when silicon melt is solidified to 85 ~ 90%, stop drawing ingot, silica tube is moved down, stretch in the not solidified excess silicon melt in upper strata, open valve, open vacuum unit, vacuum tightness in silica tube is evacuated to 1 ~ 100Pa, in vacuum chamber and silica tube, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters in silica tube completely under pressure difference effect, speed with 0.1-2mm/min continues to pull down ingot afterwards, until crucible upper end, leave behind heating zone, tailing collection box level is extended under silica tube, silica tube lower end is down to apart from tailing collection box 5 ~ 15cm,
The 3rd step aftertreatment: cut off the electricity supply, stop heating, silicon melt cooled and solidified in silica tube also expands, to after silica tube spalling, fall in tailing collection box, the tailing that is rich in impurity has just been collected among tailing collection box, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%-99.999%, and yield rate reaches 85-95%.
Described silicon material is industrial silicon, and its purity is 99.5% ~ 99.9%.
Described rare gas element is high-purity argon gas or high-purity helium, and its purity is more than 99.9%.
The equipment that a kind of method that vacuum drawn tailing carries out directional solidification purified polysilicon adopts, by vacuum chamber, form outer wall, vacuum-lines is installed on outer wall, vacuum-lines one end is connected with vacuum pump group, it is characterized in that: on outer wall, be installed with vent line, and be movably installed with tailing collection box, aqueous cold plate is movably installed in chamber bottom, graphite cake is placed in aqueous cold plate top, on graphite cake, have hole, graphite pillar one end is connected by hole and graphite cake are nested, the other end is connected with graphite pallet is nested, crucible is placed on graphite pallet, graphite heater is placed on crucible periphery and is fixed on vacuum chamber sidewall, carbon felt insulated tank is placed on outside graphite heater and is fixed on vacuum chamber sidewall, on carbon felt insulation cover, have hole, be placed in carbon felt insulated tank top, ruhmkorff coil is placed on outside carbon felt insulated tank and is fixed on vacuum chamber sidewall, silica tube is movably installed in vacuum chamber top, and its lower end is placed in central position directly over crucible through carbon felt insulation cover, upper end is connected with vacuum unit movable sealing by valve, vacuumometer is installed on vacuum unit.
Hole on described graphite cake is at least 3.
On described graphite pallet, have draw-in groove.
Between described silica tube and vacuum chamber, vacuum-sealing is flexibly connected.
Described silica tube is sharp mouth silica tube, and its lower end mouth of pipe is sharp mouth taper, and upper end is cylindrical, and integral body is the funnel shaped of upper end closed.
Described vacuum unit comprises mechanical pump and lobe pump.
The unusual effect of the inventive method is: when melt solidifying is to impurity phase during to concentrated silicon ingot top, by vacuum drawn mode, utilize pressure difference that the high tailing of foreign matter content is pressed in silica tube, fallen to afterwards on tailing collection box, reduced the back diffusion of impurity, the yield that has improved ingot casting, yield rate reaches 85%-95%, has reduced the consumption of line cutting and the cutting of diamond saw band, reduce process procedure, reduced energy consumption.
Equipment of the present invention is on the basis of original apparatus for directional solidification, to have increased silica tube, breather line and vacuum unit, scrap build is easy for installation, simple to operate, can effectively remove the impurity of ingot casting afterbody enrichment, saved production cycle and cost, be applicable to large-scale industrialization and produce.
Accompanying drawing explanation
A kind of vacuum unit of Fig. 1 extracts the equipment schematic diagram that method that tailing carries out directional solidification purified polysilicon adopts
In figure: (1) silica tube, (2) vacuum chamber, (3) carbon felt insulation cover, (4) carbon felt insulated tank, (5) ruhmkorff coil, (6) graphite heater, (7) crucible, (8) melt, (9) graphite pallet, (10) graphite pillar, (11) graphite cake, (12) aqueous cold plate, (13) tailing collection box, (14) vacuum pump group, (15) vacuum-lines, (16) vent line, (17) valve, (18) vacuum unit, (19) vacuumometer
Embodiment
Below in conjunction with specific embodiments and the drawings, describe the present invention in detail, but the present invention is not limited to specific embodiment.
Embodiment 1
The equipment that the method that a kind of vacuum drawn tailing as shown in Figure 1 carries out directional solidification purified polysilicon adopts, forms outer wall by vacuum chamber 2, and vacuum-lines 15 is installed on outer wall, and vacuum-lines one end is connected with vacuum pump group 14.
On outer wall, be installed with vent line 16, and be movably installed with tailing collection box 13, aqueous cold plate 12 is movably installed in chamber bottom, graphite cake 11 is placed in aqueous cold plate top, on graphite cake, have hole, graphite pillar 10 one end are connected by hole and graphite cake are nested, the other end is connected with graphite pallet 9 is nested, crucible is placed on graphite pallet, graphite heater 6 is placed on crucible 7 peripheries and is fixed on vacuum chamber sidewall, carbon felt insulated tank 4 is placed on outside graphite heater and is fixed on vacuum chamber sidewall, on carbon felt insulation cover 3, have hole, be placed in carbon felt insulated tank top, ruhmkorff coil 5 is placed on outside carbon felt insulated tank and is fixed on vacuum chamber sidewall.
Silica tube 1 is movably installed in vacuum chamber top, and its lower end is placed in central position directly over crucible through carbon felt insulation cover, and upper end is connected with vacuum unit 18 movable sealings by valve 17, and vacuumometer 19 is installed on vacuum unit.
Hole on graphite cake 11 is 4, on graphite pallet 9, has draw-in groove, is beneficial to graphite pillar and is connected with the nested of its.
Between silica tube 1 and vacuum chamber 2, vacuum-sealing is flexibly connected, and silica tube can move up and down and keep the effect of sealing.
Silica tube is sharp mouth silica tube, and its lower end mouth of pipe is sharp mouth taper, and upper end is cylindrical, and integral body is the funnel shaped of upper end closed.
Vacuum unit comprises mechanical pump and lobe pump.
Embodiment 2
Equipment described in employing embodiment 1 is got tailing and is carried out directional solidification purified polysilicon, first to adding the clean purity of crucible volume 90% in crucible 7, be 99.5% silicon material, close vent line 16, open vacuum pump group 14, the vacuum tightness in vacuum chamber 2 is extracted into 10Pa, close afterwards vacuum pump group, open vent line 16, in vacuum chamber 2, be filled with 99.91% argon gas, reach 100Pa to pressure, close vent line 13;
Second step melting, solidify: power-on, utilize ruhmkorff coil and graphite heater that the silicon material in crucible is heated to 1450 ℃ to being fused into silicon melt completely, and be incubated 30min at this temperature, pull vertically downward aqueous cold plate, make silicon melt in crucible with the speed of 2mm/min uniform motion vertically downward, draw ingot, silicon melt is carried out directional freeze to top by crucible bottom, when silicon melt is solidified to 85%, stop drawing ingot, silica tube is moved down, stretch in the not solidified excess silicon melt in upper strata, open valve 17, open vacuum unit 18, vacuum tightness in silica tube is evacuated to 1Pa, in vacuum chamber and silica tube, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters in silica tube completely under pressure difference effect, speed with 2mm/min continues to pull down ingot afterwards, until crucible upper end, leave behind heating zone, tailing collection box level is extended under silica tube, silica tube 1 lower end is down to apart from tailing collection box 15cm,
The 3rd step aftertreatment: cut off the electricity supply, stop heating, silicon melt cooled and solidified in silica tube 1 also expands, to after silica tube spalling, fall in tailing collection box 14, the tailing that is rich in impurity has just been collected among tailing collection box, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%, and yield rate reaches 85%.
Embodiment 3
Equipment described in employing embodiment 1 is got tailing and is carried out directional solidification purified polysilicon, first to adding the clean purity of crucible volume 93% in crucible 7, be 99.6% silicon material, close vent line 16, open vacuum pump group 14, the vacuum tightness in vacuum chamber 2 is extracted into 1Pa, close afterwards vacuum pump group, open vent line 16, in vacuum chamber 2, be filled with 99.95% argon gas, reach 1000Pa to pressure, close vent line 13;
Second step melting, solidify: power-on, utilize ruhmkorff coil and graphite heater that the silicon material in crucible is heated to 1550 ℃ to being fused into silicon melt completely, and be incubated 40min at this temperature, pull vertically downward aqueous cold plate, make silicon melt in crucible with the speed of 0.9mm/min uniform motion vertically downward, draw ingot, silicon melt is carried out directional freeze to top by crucible bottom, when silicon melt is solidified to 87%, stop drawing ingot, silica tube is moved down, stretch in the not solidified excess silicon melt in upper strata, open valve 17, open vacuum unit 18, vacuum tightness in silica tube is evacuated to 50Pa, in vacuum chamber and silica tube, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters in silica tube completely under pressure difference effect, speed with 0.9mm/min continues to pull down ingot afterwards, until crucible upper end, leave behind heating zone, tailing collection box level is extended under silica tube, silica tube 1 lower end is down to apart from tailing collection box 10cm,
The 3rd step aftertreatment: cut off the electricity supply, stop heating, silicon melt cooled and solidified in silica tube 1 also expands, to after silica tube spalling, fall in tailing collection box 14, the tailing that is rich in impurity has just been collected among tailing collection box, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.996%, and yield rate reaches 92%.
Embodiment 4
Equipment described in employing embodiment 1 is got tailing and is carried out directional solidification purified polysilicon, first to adding the clean purity of crucible volume 95% in crucible 7, be 99.9% silicon material, close vent line 16, open vacuum pump group 14, the vacuum tightness in vacuum chamber 2 is extracted into 0.01Pa, close afterwards vacuum pump group, open vent line 16, in vacuum chamber 2, be filled with 99.95% helium, reach 4000Pa to pressure, close vent line 13;
Second step melting, solidify: power-on, utilize ruhmkorff coil and graphite heater that the silicon material in crucible is heated to 1650 ℃ to being fused into silicon melt completely, and be incubated 60min at this temperature, pull vertically downward aqueous cold plate, make silicon melt in crucible with the speed of 0.1mm/min uniform motion vertically downward, draw ingot, silicon melt is carried out directional freeze to top by crucible bottom, when silicon melt is solidified to 90%, stop drawing ingot, silica tube is moved down, stretch in the not solidified excess silicon melt in upper strata, open valve 17, open vacuum unit 18, vacuum tightness in silica tube is evacuated to 100Pa, in vacuum chamber and silica tube, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters in silica tube completely under pressure difference effect, speed with 0.1mm/min continues to pull down ingot afterwards, until crucible upper end, leave behind heating zone, tailing collection box level is extended under silica tube, silica tube 1 lower end is down to apart from tailing collection box 5cm,
The 3rd step aftertreatment: cut off the electricity supply, stop heating, silicon melt cooled and solidified in silica tube 1 also expands, to after silica tube spalling, fall in tailing collection box 14, the tailing that is rich in impurity has just been collected among tailing collection box, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.999%, and yield rate reaches 95%.
Claims (10)
1. vacuum drawn tailing carries out a method for directional solidification purified polysilicon, it is characterized in that: in protection of inert gas environment, clean silicon material is heated to melt completely after forming silicon melt is incubated; Lower the temperature afterwards, draw ingot vertically downward, carry out directional freeze; When having solidified 85～90%, stop drawing ingot, silica tube is stretched in the not solidified excess silicon melt in upper strata, with vacuum unit, the silica tube the other end is vacuumized afterwards, the not solidified excess silicon melt in upper strata enters among silica tube under pressure difference effect, and until upper strata, not solidified excess silicon melt is all pressed into after silica tube, continues to pull down ingot, until crucible upper end, leave behind heating zone, tailing collection box is extended under silica tube; Cut off the electricity supply, stop heating, in silica tube, melt solidifying expands, and after silica tube spalling, with tailing, falls in tailing collection box, solidifies the ingot casting obtaining and be HIGH-PURITY SILICON ingot casting in crucible.
2. a kind of vacuum drawn tailing carries out the method for directional solidification purified polysilicon according to claim 1, it is characterized in that: the concrete steps of the method that adopts are as follows:
The first step pre-treatment: add the clean silicon material of crucible volume 90～95% in crucible (7), close vent line (16), open vacuum pump group (14), first the vacuum tightness in vacuum chamber (2) is extracted into 0.01-10Pa, close afterwards vacuum pump group, open vent line (16), in vacuum chamber (2), be filled with rare gas element, reach 100～4000Pa to pressure, close vent line (16);
Second step melting, solidify: power-on, utilize ruhmkorff coil and graphite heater that the silicon material in crucible is heated to 1450～1650 ℃ to being fused into silicon melt completely, and be incubated 30～60min at this temperature, pull vertically downward aqueous cold plate, make silicon melt in crucible with the speed of 0.1-2mm/min uniform motion vertically downward, draw ingot, silicon melt is carried out directional freeze to top by crucible bottom, when silicon melt is solidified to 85～90%, stop drawing ingot, silica tube is moved down, stretch in the not solidified excess silicon melt in upper strata, open valve (17), open vacuum unit (18), vacuum tightness in silica tube is evacuated to 1～100Pa, in vacuum chamber and silica tube, mineralization pressure is poor, the not solidified excess silicon melt in upper strata enters in silica tube completely under pressure difference effect, speed with 0.1-2mm/min continues to pull down ingot afterwards, until crucible upper end, leave behind heating zone, tailing collection box level is extended under silica tube, silica tube (1) lower end is down to apart from tailing collection box 5～15cm,
The 3rd step aftertreatment: cut off the electricity supply, stop heating, silicon melt cooled and solidified in silica tube (1) also expands, to after silica tube spalling, fall in tailing collection box (13), the tailing that is rich in impurity has just been collected among tailing collection box, in crucible, solidifying the ingot casting obtaining is HIGH-PURITY SILICON ingot casting, and its purity will reach 99.99%-99.999%, and yield rate reaches 85-95%.
3. according to the arbitrary described a kind of vacuum drawn tailing of claim 1 or 2, carry out the method for directional solidification purified polysilicon, it is characterized in that: described silicon material is industrial silicon, its purity is 99.5%～99.9%.
4. according to the arbitrary described a kind of vacuum drawn tailing of claim 1 or 2, carry out the method for directional solidification purified polysilicon, it is characterized in that: described rare gas element is high-purity argon gas or high-purity helium, and its purity is more than 99.9%.
5. the equipment that a kind of method that vacuum drawn tailing carries out directional solidification purified polysilicon according to claim 1 adopts, by vacuum chamber (2), form outer wall, vacuum-lines (15) is installed on outer wall, vacuum-lines one end is connected with vacuum pump group (14), it is characterized in that: on outer wall, be installed with vent line (16), and be movably installed with tailing collection box (13), aqueous cold plate (12) is movably installed in chamber bottom, graphite cake (11) is placed in aqueous cold plate top, on graphite cake, have hole, graphite pillar (10) one end is connected by hole and graphite cake are nested, the other end and nested connection of graphite pallet (9), crucible is placed on graphite pallet, graphite heater (6) is placed on crucible (7) periphery and is fixed on vacuum chamber sidewall, carbon felt insulated tank (4) is placed on outside graphite heater and is fixed on vacuum chamber sidewall, on carbon felt insulation cover (3), have hole, be placed in carbon felt insulated tank top, ruhmkorff coil (5) is placed on outside carbon felt insulated tank and is fixed on vacuum chamber sidewall, silica tube (1) is movably installed in vacuum chamber top, and its lower end is placed in central position directly over crucible through carbon felt insulation cover, upper end is connected with vacuum unit (18) movable sealing by valve (17), vacuumometer (19) is installed on vacuum unit.
6. the equipment that the method that a kind of vacuum drawn tailing according to claim 5 carries out directional solidification purified polysilicon adopts, is characterized in that: the hole on described graphite cake (11) is at least 3.
7. the equipment that the method that a kind of vacuum drawn tailing according to claim 5 carries out directional solidification purified polysilicon adopts, is characterized in that: on described graphite pallet (9), have draw-in groove.
8. the equipment that the method that a kind of vacuum drawn tailing according to claim 5 carries out directional solidification purified polysilicon adopts, is characterized in that: between described silica tube (1) and vacuum chamber (2), vacuum-sealing is flexibly connected.
9. the equipment that the method for carrying out directional solidification purified polysilicon according to the arbitrary described a kind of vacuum drawn tailing of claim 5 or 8 adopts, it is characterized in that: described silica tube (1) is sharp mouth silica tube, its lower end mouth of pipe is sharp mouth taper, upper end is cylindrical, and integral body is the funnel shaped of upper end closed.
10. the equipment that the method that a kind of vacuum drawn tailing according to claim 5 carries out directional solidification purified polysilicon adopts, is characterized in that: described vacuum unit (18) comprises mechanical pump and lobe pump.
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| CN103266349B (en) * | 2013-05-31 | 2015-07-15 | 大连理工大学 | High-purity hollow silicon material, as well as polycrystalline silicon and ingot silicon vacuum solid-liquid separation method and equipment |
| CN103266351B (en) * | 2013-05-31 | 2015-08-12 | 大连理工大学 | Polycrystalline silicon ingot solid-liquid separating method and equipment |
| CN103278351A (en) * | 2013-06-06 | 2013-09-04 | 青岛隆盛晶硅科技有限公司 | Sampling device for silicon melt in medium smelting, and application method thereof |
| CN112410631A (en) * | 2020-10-28 | 2021-02-26 | 西安航空学院 | Efficient single-phase Mg preparation2Method for preparing (Si, Sn) base medium temperature thermoelectric material |
| CN114457408A (en) * | 2020-12-08 | 2022-05-10 | 江苏神汇新材料科技有限公司 | Preparation method of gettering tank for cleaning impurity bottom materials in single crystal furnace |
| CN112538653A (en) * | 2020-12-08 | 2021-03-23 | 江苏神汇新材料科技有限公司 | Method for online cleaning of impurity bottom material in single crystal furnace |
| CN113584573B (en) * | 2021-08-17 | 2022-12-20 | 江苏神汇新型陶瓷材料科技有限公司 | External impurity-absorbing feeding method for single crystal furnace |
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| JP2011116616A (en) * | 2009-10-29 | 2011-06-16 | Sanki Dengyo Kk | Method for producing high-purity silicon using rotating crucible apparatus |
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| EP0477784A1 (en) * | 1990-09-20 | 1992-04-01 | Kawasaki Steel Corporation | Production of high-purity silicon ingot |
| CN101837979A (en) * | 2009-12-07 | 2010-09-22 | 耿世达 | Method for preparing solar-grade high-purity polycrystalline silicon |
| CN102219221A (en) * | 2011-06-08 | 2011-10-19 | 大连理工大学 | Method for purifying polycrystalline silicon by directional solidification and slag refining |
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